CN106085464A - Alignment film material, the manufacture method of display panels and display panels - Google Patents
Alignment film material, the manufacture method of display panels and display panels Download PDFInfo
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- CN106085464A CN106085464A CN201610388392.2A CN201610388392A CN106085464A CN 106085464 A CN106085464 A CN 106085464A CN 201610388392 A CN201610388392 A CN 201610388392A CN 106085464 A CN106085464 A CN 106085464A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
- G02F1/133711—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by organic films, e.g. polymeric films
- G02F1/133723—Polyimide, polyamide-imide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/16—Chemical modification with polymerisable compounds
- C08J7/18—Chemical modification with polymerisable compounds using wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K19/54—Additives having no specific mesophase characterised by their chemical composition
- C09K19/56—Aligning agents
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
- G02F1/13378—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by treatment of the surface, e.g. embossing, rubbing or light irradiation
- G02F1/133788—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by treatment of the surface, e.g. embossing, rubbing or light irradiation by light irradiation, e.g. linearly polarised light photo-polymerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
- G02F1/133711—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by organic films, e.g. polymeric films
Abstract
The present invention provides a kind of alignment film material, the manufacture method of display panels and display panels.The alignment film material of the present invention, prepares by being mixed in polyamic acid solution by polymerizability monomer, it is easy to make.The manufacture method of the display panels of the present invention, by described alignment film material being coated on substrate after a series of processing procedures, prepare and include Kapton and be positioned at the alignment film of multiple polymer projections on Kapton surface, this alignment film can make liquid crystal molecule vertical orientation and produce tilt angle, and there is not the risk of polymerizability monomer contamination liquid crystal molecule, promote the quality of display panels.The display panels of the present invention, simple in construction, orientation is effective, and has the display quality of excellence.
Description
Technical field
The present invention relates to Display Technique field, particularly relate to a kind of alignment film material, the manufacture method of display panels,
And display panels.
Background technology
Along with plane display dresses such as the development of Display Technique, liquid crystal displays (Liquid Crystal Display, LCD)
Put because having that high image quality, power saving, fuselage be thin and the advantage such as applied range, and be widely used in mobile phone, TV, individual number
The various consumption electronic products such as word assistant, digital camera, notebook computer, desk computer, become the master in display device
Stream.
Liquid crystal indicator major part on existing market is backlight liquid crystal display, it include display panels and
Backlight module (backlight module).The operation principle of display panels is to put in the middle of the glass substrate that two panels is parallel
Put liquid crystal molecule, have many tiny electric wires vertically and horizontally in the middle of two panels glass substrate, control liquid crystal by whether being energized
Molecular changes direction, reflects generation picture by the light of backlight module.
Generally display panels is by color film (Color Filter, CF) substrate, thin film transistor (TFT) (Thin Film
Transistor, TFT) substrate, the liquid crystal (LC, Liquid Crystal) that is sandwiched between color membrane substrates and thin film transistor base plate
And fluid sealant frame (Sealant) composition.
In TFT-LCD display, vertical orientation (Verticallyaligned, VA) display is right with its wide angle of visibility, height
Than degree with without advantages such as friction matchings, become the common pattern of large scale TV.It is vertical that vertical orientation technology is broadly divided into multidomain
Orientation (Multi-domian Vertical Alignment, MVA) technology, vertical orientated configuration (Patterned Vertial
Alignment, PVA) technology and continuous fireworks shape arrangement (Continuous pinwheel Alignment, CPA) technology.This
A little vertical orientation technology are required in the design of CF side protruding (Protrusion) or gap (Slit), while increasing cost,
Also can reduce the light transmission rate of display screen, be realized, by a control or line traffic control, the problem that face is controlled for solving CF side, create new
Vertical orientation Display Technique, is called polymer stabilizing vertical orientation (Polymer Stabilization Vertical
Alignment, PSVA) technology.
The feature of polymer stabilizing vertical orientation technology maximum is to generate one layer on alignment film to make vertical orientation liquid
The brilliant polymeric layer forming tilt angle, the formation of this one polymer is as shown in Figure 1A to Fig. 1 D, as shown in Figure 1A, at liquid crystal molecule
Mixing a certain proportion of highly purified reactive monomer (RM, Reactive Mesogen) 200 in 100, this is a kind of containing double
The phototaxis monomer of key；As shown in Figure 1B, at UV (ultraviolet) light pre-irradiation, a first additional electricity on upper and lower substrate 300,400
Pressure so that liquid crystal molecule 100 produces a tilt angle, corresponding different farmland, and the incline direction of liquid crystal molecule 100 is different；Such as figure
Shown in 1C, after determining pretilt angle with applied voltage, carrying out specific UV light and irradiate, at this moment, reactive monomer 200 aggregates into
Macromolecule network 500, attracts the liquid crystal molecule 100 on top layer to be allowed to form fixing tilt angle；As shown in figure ip, UV illumination shoots away
Cheng Hou, removes applied voltage, and the liquid crystal molecule 100 on upper and lower substrate 300,400 surface still keeps the tilt angle of certain angle.
But, reactive monomer, after UV light irradiates generation Raolical polymerizable, the most all can have part to remain
In liquid crystal, thus pollute liquid crystal, cause the appearance of ghost, reduce the quality of panel.
Summary of the invention
The primary and foremost purpose of the present invention is to provide a kind of alignment film material, can simplify the processing procedure of LCD alignment, and will not
Pollute liquid crystal, promote the quality of display panels.
Another object of the present invention is to provide the manufacture method of a kind of display panels, liquid crystal molecule can be realized vertical
Orientation also produces tilt angle, there is not the risk of polymerizability monomer contamination liquid crystal molecule in manufacturing process, promotes liquid crystal
Show the quality of panel.
A further object of the present invention is to provide a kind of display panels, and simple in construction, orientation is effective, and has excellent
Different display quality.
For achieving the above object, present invention firstly provides a kind of alignment film material, including gathering containing aromatic condensed ring structure
Amic acid, polymerisable monomer containing aromatic condensed ring structure and solvent；
The described polyamic acid containing aromatic condensed ring structure includesAndIn one or more；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit；
The described polymerisable monomer containing aromatic condensed ring structure includes AndIn one or more；
Wherein, P represents polymerizable groups, its selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy,
And at least one in epoxy radicals；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, n
During more than 1, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
The mass percent of the described polyamic acid containing aromatic condensed ring structure is 3～4%, described containing aromatic condensed ring knot
The mass percent of the polymerisable monomer of structure is 0.03～0.4%, and the mass percent of described solvent is 95.6～96.97%.
The described polyamic acid containing aromatic condensed ring structure includes
The described polymerizability monomer containing aromatic condensed ring structure includes
The present invention also provides for the manufacture method of a kind of display panels, comprises the steps:
Step 1, offer alignment film material, described alignment film material includes the polyamic acid containing aromatic condensed ring structure, contains
There are polymerisable monomer and the solvent of aromatic condensed ring structure；
The described polyamic acid containing aromatic condensed ring structure includesAndIn one or more；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit；
The described polymerisable monomer containing aromatic condensed ring structure includes AndIn one or more；
Wherein, P represents polymerizable groups, its selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy,
And at least one in epoxy radicals；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, n
During more than 1, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different；
Step 2, providing first substrate and second substrate, described first substrate includes the first underlay substrate and is located at described the
The first electrode on one underlay substrate, described second substrate includes the second underlay substrate and is located on described second underlay substrate
Second electrode；
Described in the surface-coated of the surface of the first electrode of described first substrate and the second electrode of described second substrate
The alignment film material that step 1 provides；
Described alignment film material is toasted, while making solvent fully volatilize, also makes containing aromatic condensed ring structure
Polyamic acid dehydration cyclization, be converted into the polyimides containing aromatic condensed ring structure, form Kapton, described polyamides
Imines thin film is contained within the polymerizability monomer containing aromatic condensed ring structure；
Step 3, on described first substrate or second substrate, it is provided with a dispenser method molecule of Kapton,
Described second base or the first base are provided with the peripheral applying paste of the one side correspondence liquid crystal molecule of Kapton；
Step 4, described first substrate and second substrate para-position are fitted, between described first substrate and second substrate
Liquid crystal molecule formed liquid crystal layer, fluid sealant is solidified, now, liquid crystal molecule is perpendicular to described first substrate and the second base
Plate arranges；
Step 5, apply voltage by the first electrode and the second electrode in liquid crystal layer both sides, after liquid crystal molecule deflects,
Apply while voltage, Kapton carried out UV irradiation, in Kapton containing aromatic condensed ring structure can
Polymerizable monomer, by light-initiated effect, forms multiple polymer projection at Kapton surface aggregate, thus in institute
State first substrate and second substrate surface forms the first alignment film and the second alignment film, described first alignment film and respectively
Two alignment films all include Kapton and the multiple polymer projections being positioned at Kapton surface；
Stop UV irradiating, and after removing voltage, the liquid crystal molecule near the first alignment film and the second alignment film surface produces
Tilt angle.
In the alignment film material of described step 1, the described polyamic acid containing aromatic condensed ring structure includes
The described polymerizability monomer containing aromatic condensed ring structure includes
The mass percent of the described polyamic acid containing aromatic condensed ring structure is 3～4%, described containing aromatic condensed ring knot
The mass percent of the polymerisable monomer of structure is 0.03～0.4%, and the mass percent of described solvent is 95.6～96.97%.
The preparation method of the alignment film material that described step 1 provides includes:
Step 11, the offer two anhydride monomer and the diamines monomers containing aromatic condensed ring structure, by described thick containing fragrance
Two anhydride monomers of ring structure and diamines monomer are dissolved in solvent, and reaction obtains the polyamide containing aromatic condensed ring structure
Acid, thus obtain polyamic acid solution；
Step 12, the offer polymerisable monomer containing aromatic condensed ring structure, by described gathering containing aromatic condensed ring structure
Conjunction property monomer adds in the polyamic acid solution that described step 11 prepares, and prepares alignment film material.
In described step 5, liquid crystal layer both sides apply voltage be 13～25V, UV irradiate time UV light light intensity be 85～
100mW/cm2, irradiation time is 20～30min.
The present invention also provides for a kind of display panels, including the first substrate being oppositely arranged and second substrate, is located at institute
State the liquid crystal layer between first substrate and second substrate, be located on first substrate near liquid crystal layer side the first alignment film, with
And it is located on second substrate the second alignment film near liquid crystal layer side；
Described first, second the first alignment films and the second alignment film all include Kapton and are positioned at polyimides
Multiple polymer projections of film surface；
The material of described Kapton includes the polyimides containing aromatic condensed ring structure, described containing aromatic condensed ring
The polyimides of structure includesAndIn one or more, its
In, x >=1；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit；
Described polymer projection is polymerized by the polymerisable monomer containing aromatic condensed ring structure, described containing aromatic condensed ring knot
The polymerisable monomer of structure includes
AndIn one or more；
P represents polymerizable groups, and it is selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy and ring
At least one in epoxide；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, and n is more than 1
Time, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
The described polyimides containing aromatic condensed ring structure includes
The described polymerizability monomer containing aromatic condensed ring structure includes
Beneficial effects of the present invention: a kind of alignment film material that the present invention provides, by being mixed into poly-by polymerizability monomer
Amic acid solution prepares, it is easy to make.The manufacture method of a kind of display panels that the present invention provides, by joining described
Coat on substrate after a series of processing procedures to membrane material, prepare and include Kapton and be positioned at Kapton table
The alignment film of multiple polymer projections in face, this alignment film can make liquid crystal molecule vertical orientation and produce tilt angle, and not depositing
In the risk of polymerizability monomer contamination liquid crystal molecule, promote the quality of display panels.A kind of liquid crystal that the present invention provides
Display floater, simple in construction, orientation is effective, and has the display quality of excellence.
In order to be able to be further understood that inventive feature and technology contents, refer to below in connection with the present invention is detailed
Illustrate and accompanying drawing, but accompanying drawing only provides reference and explanation use, be not used for the present invention is any limitation as.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings, by the detailed description of the invention of the present invention is described in detail, technical scheme will be made
And other beneficial effect is apparent.
In accompanying drawing,
Figure 1A-1D is the processing procedure schematic diagram of existing polymer vertical orientation technology；
Fig. 2 is the flow chart of the manufacture method of the display panels of the present invention；
Fig. 3 is the schematic diagram of step 2-4 of the manufacture method of the display panels of the present invention；
Fig. 4-5 is the schematic diagram of the step 5 of the manufacture method of the display panels of the present invention and Fig. 5 is the liquid of the present invention
The structural representation of LCD panel.
Detailed description of the invention
By further illustrating the technological means and effect, being preferable to carry out below in conjunction with the present invention that the present invention taked
Example and accompanying drawing thereof are described in detail.
Present invention firstly provides a kind of alignment film material, including the polyamic acid containing aromatic condensed ring structure, containing fragrance
The polymerisable monomer of condensed cyclic structure and solvent；
The described polyamic acid containing aromatic condensed ring structure includesAndIn one or more, wherein, x is 20～10000；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit.
Concrete, described annular unit includes five-membered ring and one or more in hexatomic ring；Described hexatomic ring includes virtue
One or more in fragrant ring and cycloaliphatic ring.
Preferably,IncludingAndIn one or more
Combination.
Preferably, the described polyamic acid containing aromatic condensed ring structure includes
Wherein, x is 20～10000.
The described polymerisable monomer containing aromatic condensed ring structure includes AndIn one or more；
Wherein, P represents polymerizable groups, its selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy,
And at least one in epoxy radicals；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, n
During more than 1, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different；
It will be appreciated by those skilled in the art that, on same aromatic rings, n+m certainly less than or equal to this aromatic rings
Total number of upper attachable group.
Preferably, the described polymerizability monomer containing aromatic condensed ring structure includes
Concrete, described solvent includes N-Methyl pyrrolidone (NMP), N-ethyl pyrrolidine, γ-hexalactone, dimethyl
One or more of sulfoxide and dichloromethane.Preferably, described solvent is N-Methyl pyrrolidone.
Concrete, the mass percent of the described polyamic acid containing aromatic condensed ring structure is 3～4%, described containing virtue
The mass percent of the polymerisable monomer of fragrant condensed cyclic structure is 0.03～0.4%, the mass percent of described solvent be 95.6～
96.97%.
Referring to Fig. 2, the present invention provides the manufacture method of a kind of display panels, comprises the steps:
Step 1, offer alignment film material, described alignment film material includes the polyamic acid containing aromatic condensed ring structure, contains
There are polymerisable monomer and the solvent of aromatic condensed ring structure.
Concrete, the described polyamic acid containing aromatic condensed ring structure includes
AndIn one or more, wherein, x is 20～10000；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit.
Concrete, described annular unit includes five-membered ring and one or more in hexatomic ring；Described hexatomic ring includes virtue
One or more in fragrant ring and cycloaliphatic ring.
Preferably,IncludingAndIn one or
Multiple combination.
Concrete, the described polymerisable monomer containing aromatic condensed ring structure includes AndIn one
Or it is multiple；
Wherein, P represents polymerizable groups, its selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy,
And at least one in epoxy radicals；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, n
During more than 1, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
Concrete, in described alignment film material, the mass percent of the described polyamic acid containing aromatic condensed ring structure is 3
～4%, the mass percent of the described polymerisable monomer containing aromatic condensed ring structure is 0.03～0.4%, the matter of described solvent
Amount percentage ratio is 95.6～96.97%.
Concrete, the preparation method of the alignment film material that described step 1 provides includes:
Step 11, the offer two anhydride monomer and the diamines monomers containing aromatic condensed ring structure, by described thick containing fragrance
Two anhydride monomers of ring structure and diamines monomer are dissolved in solvent, and reaction obtains the polyamide containing aromatic condensed ring structure
Acid, thus obtain polyamic acid solution.
Concrete, in described step 11, the described two anhydride monomers containing aromatic condensed ring structure are pressed with diamines monomer
It is dissolved in solvent according to the ratio that mol ratio is 1:1.Concrete, described step 11 is at room temperature carried out, the response time be 20～
30 hours, preferably 24 hours.
Concrete, the general structure of the described two anhydride monomers containing aromatic condensed ring structure isIts
In,IncludingAndIn
The combination of one or more.
Preferably, the described two anhydride monomers containing aromatic condensed ring structure are
Concrete, described diamines monomer includes the diamines monomer containing aromatic condensed ring structure and without aromatic condensed ring
At least one in structure diamines monomer.
Concrete, the general structure of the described diamines monomer containing aromatic condensed ring structure is
Wherein,Including AndIn
The combination of one or more.
Preferably, the described diamines monomer containing aromatic condensed ring structure is
Concrete, the described general structure without aromatic condensed ring structure diamines monomer isIts
In,For comprising the non-aromatic condensed ring class group of annular unit.
Concrete, described annular unit includes five-membered ring and one or more in hexatomic ring；Described hexatomic ring includes virtue
One or more in fragrant ring and cycloaliphatic ring.
Preferably,IncludingAndIn one or
Multiple combination.
Concrete, containing two anhydride monomers of aromatic condensed ring structureWith containing aromatic condensed ring structure
Diamines monomerThe reaction equation of the polyamic acid that the generation that reacts contains aromatic condensed ring structure is:
The polyamic acid containing aromatic condensed ring structure that above-mentioned reaction obtains is
Wherein, x is 20～10000.
Concrete, described solvent includes N-Methyl pyrrolidone (NMP), N-ethyl pyrrolidine, γ-hexalactone, dimethyl
One or more of sulfoxide and dichloromethane.Preferably, described solvent is N-Methyl pyrrolidone.
Step 12, the offer polymerisable monomer containing aromatic condensed ring structure, by described gathering containing aromatic condensed ring structure
Conjunction property monomer adds in the polyamic acid solution that described step 11 prepares, and prepares alignment film material.
Concrete, in described step 12, according in the described polymerizability monomer containing aromatic condensed ring structure and step 11
The two anhydride monomers containing aromatic condensed ring structure added or the mol ratio of diamines monomer be 0.5～10% ratio by institute
State the polymerizability monomer containing aromatic condensed ring structure to add in described polyamic acid solution.
Concrete, the described polymerisable monomer containing aromatic condensed ring structure includes AndIn one
Or it is multiple；
Wherein, P represents polymerizable groups, its selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy,
And at least one in epoxy radicals；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, n
During more than 1, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
Preferably, the described polymerizability monomer containing aromatic condensed ring structure includes
The polymerizability monomer containing aromatic condensed ring structure that the present invention selects, with traditional polymer vertical orientation technology
The methyl acrylic ester polymerizability monomer containing phenyl ring selected is compared, and has higher thermostability and higher photoreaction
Ability.
Step 2, refer to Fig. 3, it is provided that first substrate 10 and second substrate 20, described first substrate 10 includes the first substrate
Substrate 11 includes the second underlay substrate 21 with the first electrode 12 being located on described first underlay substrate 11, described second substrate 20
With the second electrode 22 being located on described second underlay substrate 21；
On the surface of the first electrode 12 of described first substrate 10 and the surface of the second electrode 22 of described second substrate 20
Coat the alignment film material that described step 1 provides；
Described alignment film material is toasted, while making solvent fully volatilize, also makes containing aromatic condensed ring structure
Polyamic acid dehydration cyclization, be converted into the polyimides containing aromatic condensed ring structure, form Kapton 50, described poly-
Imide membrane 50 is contained within the polymerizability monomer containing aromatic condensed ring structure.
Concrete, in described step 2, under the temperature conditions of 180～200 DEG C, described alignment film material is toasted,
Baking time is 20min-60min, preferably 30min.
Concrete, the polyimides containing aromatic condensed ring structure that described step 2 obtains includesAndIn one or more, wherein, x is 20～10000；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit.
Concrete, described annular unit includes five-membered ring and one or more in hexatomic ring；Described hexatomic ring includes virtue
One or more in fragrant ring and cycloaliphatic ring.
Preferably,IncludingAndIn one or more
Combination.
Concrete, containing the polyamic acid of aromatic condensed ring structureDehydration
The reaction equation being converted into the polyimides containing aromatic condensed ring structure is:
The polyimides containing aromatic condensed ring structure that above-mentioned reaction obtains isWherein,
X is 20～10000.
By introducing the A group containing aromatic condensed ring structure in polyimides, Kapton 50 can be strengthened and absorb
The ability of light, improves the control ability to polymerizability monomer, can also improve the thermostability of Kapton 50 simultaneously.
Due to the polarity of the described polyimides containing aromatic condensed ring structure be better than described containing aromatic condensed ring structure can
The polarity of polymerization monomer, therefore the two can produce separated, and the described polymerisable monomer containing aromatic condensed ring structure tends to gather
Combine in the surface of described Kapton 50.
Step 3, refer to Fig. 3, described first substrate 10 or second substrate 20 are provided with the one of Kapton 50
Face dispenser method molecule, is provided with the one side correspondence liquid crystal of Kapton 50 on described second substrate 20 or first substrate 10
The peripheral applying paste 40 of molecule.
Preferably, described step 3 is additionally included on described second substrate 20 or first substrate 10 outside corresponding fluid sealant 40
Enclose applying conductive glue.
Step 4, refer to Fig. 3, described first substrate 10 is fitted with second substrate 20 para-position, is positioned at described first substrate
Liquid crystal molecule between 10 and second substrate 20 forms liquid crystal layer 30, solidifies fluid sealant 40, and now, liquid crystal molecule is vertical
Arrange with second substrate 20 in described first substrate 10.
Concrete, in described step 4, under vacuum conditions described first substrate 10 is fitted with second substrate 20 para-position.
Concrete, in described step 4, the method solidifying fluid sealant 40 includes in heat cure and UV solidification
Plant or multiple.
Step 5, refer to Fig. 4-5, apply voltage by the first electrode 12 and the second electrode 22 in liquid crystal layer 30 both sides, treat
After liquid crystal molecule deflection, while applying voltage, Kapton 50 is carried out UV irradiation, in Kapton 50
Polymerizability monomer containing aromatic condensed ring structure, by light-initiated effect, is formed many at Kapton 50 surface aggregate
Individual polymer projection 60, thus form the first alignment film 61 and respectively at described first substrate 10 and second substrate 20 surface
Two alignment films 62, described first alignment film 61 and the second alignment film 62 all include Kapton 50 and are positioned at polyimides
Multiple polymer projections 60 on thin film 50 surface；
Stop UV irradiating, and after removing voltage, near the first alignment film 61 and liquid crystal molecule on the second alignment film 62 surface
Produce tilt angle.
Concrete, in described step 5, the plurality of polymer projection 60 plays maintenance the first alignment film 61 and second and joins
The effect of the deflection angle of the liquid crystal molecule to film 62 surface.
Concrete, in described step 5, the voltage applied in liquid crystal layer 30 both sides is 13～25V, the light of UV light when UV irradiates
It is by force 85～100mW/cm2, irradiation time is 20～30min.
Concrete, in described step 5, the tilt angle of described liquid crystal molecule is 0.5 °～2 °.
The manufacture method of the display panels of the present invention, by being mixed into polymerizability monomer in polyamic acid solution,
Prepare alignment film material, alignment film material is coated and obtains containing the polymerizable containing aromatic condensed ring structure after baking on substrate
The Kapton of property monomer, after Kapton is carried out UV irradiation, polymerizability monomer is at Kapton table
Face polymerization forms polymer projection, makes liquid crystal molecule produce tilt angle, it is achieved orientation effect under the mating reaction of voltage, with poly-
Compound vertical orientation technology is compared, and the present invention need not be mixed into polymerizability monomer in liquid crystal molecule, it is to avoid after UV photoreaction
The polymerizability monomer contamination liquid crystal molecule of residual, promote the quality of display panels.
Referring to Fig. 5, manufacture method based on above-mentioned display panels, the present invention also provides for a kind of LCD
Plate, including the first substrate 10 being oppositely arranged and second substrate 20, is located between described first substrate 10 and second substrate 20
Liquid crystal layer 30, it is located on first substrate 10 near the first alignment film 61 of liquid crystal layer 30 side and is located on second substrate 20
The second alignment film 62 near liquid crystal layer 30 side；
Described first alignment film 61 and the second alignment film 62 all include Kapton 50 and are positioned at Kapton
Multiple polymer projections 60 on 50 surfaces；
The material of described Kapton 50 includes the polyimides containing aromatic condensed ring structure, described thick containing fragrance
The polyimides of ring structure includesAndIn one or more,
Wherein, x is 20～10000；
Wherein,All include AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit.
Concrete, described annular unit includes five-membered ring and one or more in hexatomic ring；Described hexatomic ring includes virtue
One or more in fragrant ring and cycloaliphatic ring.
Preferably,IncludingAndIn one or
Multiple combination.
Preferably, the described polyimides containing aromatic condensed ring structure includes
By introducing in polyimides, there is aromatic condensed ring structureGroup, can strengthen
The light absorbing ability of Kapton 50, improves the control ability to polymerizability monomer, can also improve polyamides sub-simultaneously
The thermostability of amine thin film 50.
Described polymer projection 60 is polymerized by the polymerisable monomer containing aromatic condensed ring structure, described thick containing fragrance
The polymerisable monomer of ring structure includes
AndIn one or more；
P represents polymerizable groups, and it is selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy and ring
At least one in epoxide；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, and n is more than 1
Time, n polymerizable groups P is identical or different；
X represents substituted radical, its selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom,
And at least one in the group that in this alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on one aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
Preferably, the described polymerizability monomer containing aromatic condensed ring structure includes
By aromatic condensed ring structure being incorporated in polymerizability monomer, the thermostability of polymerizability monomer can be promoted, with
The photoreaction ability of Shi Tigao polymerizability monomer.
Concrete, described first substrate 10 includes the first underlay substrate 11 and is located at described first underlay substrate 11 and the
The first electrode 12 between one alignment film 61, described second substrate 20 includes the second underlay substrate 21 and is located at described second lining
The second electrode 22 between substrate 21 and the second alignment film 62.
Concrete, described display panels also includes being located between described first substrate 10 and second substrate 20 and being positioned at
The fluid sealant 40 of described liquid crystal layer 30 periphery.
Preferably, described display panels also includes being located between described first substrate 10 and second substrate 20 and being positioned at
The conducting resinl of described fluid sealant 40 periphery.
The display panels of the present invention, simple in construction, orientation is effective, and has the display quality of excellence.
In sum, the present invention provides a kind of alignment film material, the manufacture method of display panels and LCD
Plate.The alignment film material of the present invention, prepares by being mixed in polyamic acid solution by polymerizability monomer, it is easy to make.This
The manufacture method of bright display panels, by described alignment film material is coated on substrate after a series of processing procedures,
Preparing and include Kapton and be positioned at the alignment film of multiple polymer projections on Kapton surface, this alignment film can
So that liquid crystal molecule vertical orientation produce tilt angle, and there is not the risk of polymerizability monomer contamination liquid crystal molecule, promote
The quality of display panels.The display panels of the present invention, simple in construction, orientation is effective, and has the display of excellence
Quality.
The above, for the person of ordinary skill of the art, can be according to technical scheme and technology
Other various corresponding changes and deformation are made in design, and all these change and deformation all should belong to the claims in the present invention
Protection domain.
Claims (10)
1. an alignment film material, it is characterised in that include the polyamic acid containing aromatic condensed ring structure, tie containing aromatic condensed ring
The polymerisable monomer of structure and solvent；
The described polyamic acid containing aromatic condensed ring structure includesAndIn one or more；
Wherein,All include
AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit；
The described polymerisable monomer containing aromatic condensed ring structure includes AndIn one or more；
Wherein, P represents polymerizable groups, and it is selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy and ring
At least one in epoxide；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, and n is more than 1
Time, n polymerizable groups P is identical or different；
X represents substituted radical, and it is selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom and is somebody's turn to do
At least one in the group that in alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
2. alignment film material as claimed in claim 1, it is characterised in that the described polyamic acid containing aromatic condensed ring structure
Mass percent is 3～4%, and the mass percent of the described polymerisable monomer containing aromatic condensed ring structure is 0.03～0.4%,
The mass percent of described solvent is 95.6～96.97%.
3. alignment film material as claimed in claim 1, it is characterised in that the described polyamic acid bag containing aromatic condensed ring structure
Include
The described polymerizability monomer containing aromatic condensed ring structure includes
4. the manufacture method of a display panels, it is characterised in that comprise the steps:
Step 1, offer alignment film material, described alignment film material includes the polyamic acid containing aromatic condensed ring structure, containing virtue
The polymerisable monomer of fragrant condensed cyclic structure and solvent；
The described polyamic acid containing aromatic condensed ring structure includesAndIn one or more；
Wherein,All include
AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit；
The described polymerisable monomer containing aromatic condensed ring structure includes AndIn one or more；
Wherein, P represents polymerizable groups, and it is selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy and ring
At least one in epoxide；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, and n is more than 1
Time, n polymerizable groups P is identical or different；
X represents substituted radical, and it is selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom and is somebody's turn to do
At least one in the group that in alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different；
Step 2, offer first substrate (10) and second substrate (20), described first substrate (10) includes the first underlay substrate (11)
With the first electrode (12) being located on described first underlay substrate (11), described second substrate (20) includes the second underlay substrate
(21) with the second electrode (22) being located on described second underlay substrate (21)；
The second electrode (22) at the surface of the first electrode (12) of described first substrate (10) and described second substrate (20)
The alignment film material that step 1 described in surface-coated provides；
Described alignment film material is toasted, while making solvent fully volatilize, also makes gathering containing aromatic condensed ring structure
Amic acid dehydration cyclization, is converted into the polyimides containing aromatic condensed ring structure, forms Kapton (50), described polyamides
Imines thin film (50) is contained within the polymerizability monomer containing aromatic condensed ring structure；
Step 3, on described first substrate (10) or second substrate (20), it is provided with the one side drip liquid of Kapton (50)
Brilliant molecule, the one side correspondence liquid crystal being provided with Kapton (50) on described second substrate (20) or first substrate (10) divides
The peripheral applying paste (40) of son；
Step 4, described first substrate (10) and second substrate (20) para-position are fitted, be positioned at described first substrate (10) and second
Liquid crystal molecule between substrate (20) forms liquid crystal layer (30), solidifies fluid sealant (40), and now, liquid crystal molecule is perpendicular to
Described first substrate (10) arranges with second substrate (20)；
Step 5, apply voltage by the first electrode (12) and the second electrode (22) in liquid crystal layer (30) both sides, treat that liquid crystal molecule is inclined
After Zhuaning, while applying voltage, Kapton (50) carrying out UV irradiation, containing in Kapton (50) is fragrant
The polymerizability monomer of fragrant condensed cyclic structure, by light-initiated effect, is formed multiple poly-at Kapton (50) surface aggregate
Compound protruding (60), thus described first substrate (10) and second substrate (20) surface formed respectively the first alignment film (61),
And second alignment film (62), described first alignment film (61) and the second alignment film (62) all include Kapton (50) with
It is positioned at multiple polymer projections (60) on Kapton (50) surface；
Stop UV irradiating, and after removing voltage, near the first alignment film (61) and the liquid crystal molecule on the second alignment film (62) surface
Produce tilt angle.
5. the manufacture method of display panels as claimed in claim 4, it is characterised in that the alignment film material of described step 1
In material, the described polyamic acid containing aromatic condensed ring structure includes
The described polymerizability monomer containing aromatic condensed ring structure includes
6. the manufacture method of display panels as claimed in claim 4, it is characterised in that described containing aromatic condensed ring structure
The mass percent of polyamic acid be 3～4%, the mass percent of the described polymerisable monomer containing aromatic condensed ring structure is
0.03～0.4%, the mass percent of described solvent is 95.6～96.97%.
7. the manufacture method of display panels as claimed in claim 4, it is characterised in that the orientation that described step 1 provides
The preparation method of membrane material includes:
Step 11, the offer two anhydride monomer and the diamines monomers containing aromatic condensed ring structure, tie described containing aromatic condensed ring
Two anhydride monomers of structure and diamines monomer are dissolved in solvent, and reaction obtains the polyamic acid containing aromatic condensed ring structure, from
And obtain polyamic acid solution；
Step 12, the offer polymerisable monomer containing aromatic condensed ring structure, by the described polymerizability containing aromatic condensed ring structure
Monomer adds in the polyamic acid solution that described step 11 prepares, and prepares alignment film material.
8. the manufacture method of display panels as claimed in claim 4, it is characterised in that in described step 5, at liquid crystal layer
(30) voltage that both sides apply is 13～25V, and when UV irradiates, the light intensity of UV light is 85～100mW/cm2, irradiation time be 20～
30min。
9. a display panels, it is characterised in that include the first substrate (10) being oppositely arranged and second substrate (20), set
Liquid crystal layer (30) between described first substrate (10) and second substrate (20), to be located at first substrate (10) upper near liquid crystal layer
(30) first alignment film (61) of side and be located at upper the second alignment film near liquid crystal layer (30) side of second substrate (20)
(62)；
Described first alignment film (61) and the second alignment film (62) all include Kapton (50) and to be positioned at polyimides thin
Multiple polymer projections (60) on film (50) surface；
The material of described Kapton (50) includes the polyimides containing aromatic condensed ring structure, described containing aromatic condensed ring
The polyimides of structure includesAndIn one or more；
Wherein,All include
AndIn the combination of one or more,WithIdentical or different；
For comprising the non-aromatic condensed ring class group of annular unit；
Described polymer projection (60) is polymerized by the polymerisable monomer containing aromatic condensed ring structure, described containing aromatic condensed ring
The polymerisable monomer of structure includes
AndIn one or more；
P represents polymerizable groups, and it is selected from methacrylic acid ester group, acrylate-based, vinyl, ethyleneoxy and epoxy radicals
In at least one；N is the number of the polymerizable groups P being connected on same aromatic rings, n=1,2 or 3, when n is more than 1, and n
Individual polymerizable groups P is identical or different；
X represents substituted radical, and it is selected from-F ,-Cl ,-Br, methyl ,-CN, the straight or branched alkyl of 2-8 carbon atom and is somebody's turn to do
At least one in the group that in alkyl, one or more methyl obtain after being replaced by oxygen or sulphur atom；M is same for being connected to
The number of the substituted radical X on aromatic rings, m=1,2 or 3, when m is more than 1, m substituted radical X is identical or different.
10. display panels as claimed in claim 9, it is characterised in that the described polyamides containing aromatic condensed ring structure is sub-
Amine includes
The described polymerizability monomer containing aromatic condensed ring structure includes
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| CN201610388392.2A CN106085464B (en) | 2016-06-02 | 2016-06-02 | Alignment film material, the production method of liquid crystal display panel and liquid crystal display panel |
| PCT/CN2016/086537 WO2017206204A1 (en) | 2016-06-02 | 2016-06-21 | Alignment film material, liquid crystal display panel manufacturing method, and liquid crystal display panel |
| US15/116,225 US10168580B2 (en) | 2016-06-02 | 2016-06-21 | Material of alignment films, methods of fabricating liquid crystal display panels and liquid crystal display panels |
| US16/197,293 US10663805B2 (en) | 2016-06-02 | 2018-11-20 | Material of alignment films, methods of fabricating liquid crystal display panels and liquid crystal display panels |
| US16/197,282 US10690966B2 (en) | 2016-06-02 | 2018-11-20 | Material of alignment films, methods of fabricating liquid crystal display panels and liquid crystal display panels |
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| CN201610388392.2A CN106085464B (en) | 2016-06-02 | 2016-06-02 | Alignment film material, the production method of liquid crystal display panel and liquid crystal display panel |
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Also Published As
| Publication number | Publication date |
|---|---|
| US10663805B2 (en) | 2020-05-26 |
| US20190086737A1 (en) | 2019-03-21 |
| US10168580B2 (en) | 2019-01-01 |
| US20190107757A1 (en) | 2019-04-11 |
| WO2017206204A1 (en) | 2017-12-07 |
| US20170371207A1 (en) | 2017-12-28 |
| CN106085464B (en) | 2019-01-15 |
| US10690966B2 (en) | 2020-06-23 |
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